Synthesizing method of nafcillin acid
A technology of nafcillin acid and synthesis method, which is applied in the field of semi-synthetic antibiotic nafcillin sodium, can solve the problems of great influence on the yield of the target product, cumbersome and complicated operation process, and physical hazards of operators, so as to reduce human harm and environmental pollution, avoid repeated phase separation, and reduce the effect of labor
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Embodiment 1
[0021] Add 45kg of 6-APA to the reaction tank with 90L of purified water, cool down to 0°C, add 225L of 3.7% sodium hydroxide solution in a trickle, after 6-APA is dissolved and clarified, add 1-chloroformyl-2 in 10min - 45kg of ethoxynaphthalene solids, during the addition of 1-chloroformyl-2-ethoxynaphthalene solids, use 3.7% sodium hydroxide solution to control the pH value of the reaction solution at 7.0, and keep the reaction at 20°C for 15 minutes after the addition is complete . Add 2kg of activated carbon, stir for 20min, filter the activated carbon, add 78kg of butyl acetate to the filtrate, cool down to 0-10°C, acidify with 3% dilute sulfuric acid to pH=1.5-2.0, precipitate crystals, continue to stir for 1h, shake off, filter with purified water Wash the crystals until the pH of the washing solution is 4.0, dry the washed filter cake, put it on a plate, put it in a vacuum drying oven at 45-55°C, and dry it to a moisture content of 2.4% to obtain 77.8 kg of nafcillin ...
Embodiment 2
[0023] Add 45kg of 6-APA to the reaction tank with 180L of purified water, cool down to 5°C, add 220L of 8% sodium bicarbonate solution in a trickle, after 6-APA is dissolved and clarified, add 1-chloroformyl-2 in batches within 13 minutes -Ethoxynaphthalene solid 47.3kg, during the addition of 1-chloroformyl-2-ethoxynaphthalene solid, use 8% sodium bicarbonate solution to control the pH value of the reaction solution at 7.2, after the addition is completed, keep the reaction at 18°C for 20min . Add 2 kg of activated carbon, stir for 20 minutes, filter the activated carbon, add 68 kg of n-hexane to the filtrate, cool down to 0-10°C, acidify with 5% dilute hydrochloric acid to pH 1.5-2.0, precipitate crystals, continue to stir for 1 hour, and filter with purified water Wash the crystals until the pH of the washing solution is 4.0, dry the washed filter cake, put it into a tray, put it in a vacuum drying oven at 45-55°C, and dry it to a moisture content of 2.0% to obtain 78.6 ...
Embodiment 3
[0025] Add 45kg of 6-APA to the reaction tank with 220L of purified water, cool down to 3°C, add 220L of 5% sodium carbonate solution in a trickle, after 6-APA is dissolved and clarified, add 1-chloroformyl-2- 49.5 kg of ethoxynaphthalene solids, during the addition of 1-chloroformyl-2-ethoxynaphthalene solids, use 5% sodium carbonate solution to control the pH value of the reaction solution at 6.8, and keep the reaction at 15°C for 30 minutes after the addition is complete. Add 2 kg of activated carbon, stir for 20 minutes, filter the activated carbon, add 73 kg of ethyl acetate to the filtrate, cool down to 0-10 ° C, acidify with 2% dilute phosphoric acid to pH 1.5-2.0, precipitate crystals, continue stirring for 1 hour, shake off the filter, and purify Wash the crystals with water until the pH of the washing solution is 4.0, dry the washed filter cake, put it on a plate, put it in a vacuum drying oven at 45-55°C, and dry it to a moisture content of 1.8%, to obtain 78.3 kg of...
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